Reaktion #77577

Reaktionsgleichung

1,4-bis[5-(3,4,5-triethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine

methanesulfonic acid

→

title compound

Ausbeute 94.0%

1,4-Bis[5-(3,4,5-triethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine Dimethanesulfonate

Ausbeute 94.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONEthanol (5.0 mL) was added to the residue
3. 3
   Einengenthe resulting mixture was concentrated under reduced pressure
4. 4
   SonstigeThe residue was recrystallized from methanol-diethyl ether

Vorschrift

To a solution of 1,4-bis[5-(3,4,5-triethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (77 mg, 0.115 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.23 mL, 0.23 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a pale yellow crystalline powder (melting point: 235.0-237.0° C.) (74.0 mg, yield: 94%).

Quelle